• 한국근적외분광분석학회:학술대회논문집
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• 한국근적외분광분석학회 2002년도 강연요지집
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• pp.97-117
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• 2002

A chemoinfometrical method for quantitative determination of crystal content of indomethacin (IMC) polymorphs based on fourie-transformed near-infrared (FT-NIR) spectroscopy was established. A direct comparison of the data with the ones collected from using the conventional powder X-ray diffraction method was performed. Pure $\alpha$ and ${\gamma}$ forms of IMC were prepared using published methods. Powder X-ray diffraction profiles and NIR spectra were recorded for six kinds of standard materials with various content of ${\gamma}$ form IMC. The principal component regression (PCR) analyses were performed based on normalized NIR spectra sets of standard samples of known content of IMC ${\gamma}$ form. A calibration equation was determined to minimize the root mean square error of the prediction. The predicted ${\gamma}$ form content values were reproducible and had a relatively small standard deviation. The values of ${\gamma}$ form content predicted by two methods were in close agreement. The results were indicated that NIR spectroscopy provides for an accurate quantitative analysis of crystallinity in polymorphs compared with the results obtained by conventional powder X-ray diffractometry.

• 통합자연과학논문집
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• 제9권2호
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• pp.94-102
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• 2016

The crystal structure of the potential active 6-ethoxy-3-phenyl-5a,9a-dihydro-3H-chromen[4,3-c][1,2]oxazole-3a(4H)-carbonitrile ($C_{19}H_{15}N_2O_3$) has been determined from single crystal X-ray diffraction technique. The title compound crystallizes in the monoclinic space group C2/c with unit cell dimension a= 29.3026(9) ${\AA}$, b= 6.7695(2) ${\AA}$ and c= 19.7597(6) ${\AA}$ [${\alpha}= 90^{\circ}$, ${\beta}= 125.709(10)^{\circ}$ and ${\gamma}= 90^{\circ}$]. Single crystals suitable for X-ray diffraction were obtained by slow evaporation method, the isoxazole and six membered pyran rings adopts envelope conformation. The crystal packing of the molecules is stabilized by the weak $C-H{\ldots}N$ hydrogen bond interaction.

• 통합자연과학논문집
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• 제9권2호
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• pp.103-112
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• 2016

The crystal structure of the potential active Methyl 8-bromo-3-phenyl-5a,9a-dihydro-3H-chromen [4,3-c][1,2] isoxazole-3a(4H)-carboxylate ($C_{18}H_{15}BrNO_4$) has been determined from single crystal X-ray diffraction technique. The title compound crystallizes in the triclinic space group Pī with unit cell dimension a=8.3129 (3) ${\AA}$, b=9.5847 (4) ${\AA}$ and c=11.1463(4) ${\AA}$ [${\alpha}=98.457(3)^{\circ}$, ${\beta}=102.806(2)^{\circ}$ and ${\gamma}=105.033(5)^{\circ}$]. Single crystals suitable for X-ray diffraction were obtained by slow evaporation method, the isoxazole and six membered pyran rings adopts envelope conformation. In the crystal, molecules are linked via pairs of inter molecular $C-H{\ldots}O$ hydrogen bonds to form dimmers.

• 한국자기학회지
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• 제8권4호
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• pp.203-209
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• 1998

Single phase garmet Y3-xBixFe5O12(x=0.0, 0.25, 0.5, 0.75, 1.0)을 ethylene glycol을 용매로 하여 sol-gel 법으로 합성후 x-ray diffraction, Mossbauer 분광기, vibrating sample magnetometer (VSM)를 이용하여 결정학적 및 자기적 특성을 연구하였다. Y과 Fe의 수화 반응을 통하여 얻은 Y3Fe5O12의 x-ray 회절 분석 결과는 결정구조가 cubic임을 알 수 있었고 Y에 Bi를 치환한 경우 또한 cubic 구조이었으며 Bi의 치환 량이 증가할수록 격자 상수가 선형적으로 증가함을 알수 있었다. Bi를 첨가한 Y3-xBixFe5O12 (x=0.0, 0.25, 0.5, 0.75, 1.0)의 단일상의 garnet이 형성되기 시작하는 온도는 80$0^{\circ}C$이고 secound phase (BiFeO3)가 생성되기 시작하는 온도는 x=0.75는 100$0^{\circ}C$이며 x-1.0은 95$0^{\circ}C$였다. Mossbauer 분광 실험과 VSM측정 결과 Birk 치환 될수록 포화 자화 값과 coercivity값이 감소하는 경향을 보였으며 Curic 온도는 Bi의 치환 양이 증가할수록 약간 증가하는 경향을 보임을 알 수 있었다.

• 한국세라믹학회지
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• 제34권10호
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• pp.1045-1052
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• 1997

Barium ferrites (BaFe12O19) were synthesized at the various temperature by the coprecipitation-oxidation method. X-ray diffraction Rietveld analysis for barium ferrites were performed, their microstructures were observed and their magnetic properties were measured, in order to analyze the crystal structures and determine the optimal temperature of heat-treatment. The barium ferrite, its average particle size 80 nm, was formed at 600℃ through the hematite (α-Fe2O3), but the site occupations of the Fe's in tetrahedral and bipyramidal sites and of the Ba relatively low. Increasing the heating temperature, these occupations and the magnetization increased, and the crystal c-axis decreased. These changes were very small at the heat treatment of above 800℃, but the particles were rapidly grown. It is suggested that the optimal temperature of heat-treatment is 800℃, at which temperature crystal structure is relatively stable and the particles hardly ever grow.

• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 2005년도 하계학술대회 논문집 Vol.6
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• pp.313-314
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• 2005

$PbTiO_3$ and PZT(52/48) powders, prepared by the sol-gel method, were mixed with an organic vehicle and the PT/PZT(52/40) heterolayered thick films were fabricated by the screen-printing method on Pt/$Al_2O_3$ substrates. The structural properties such as DTA, X-ray diffraction and microstructure, were examined as a amount of the PbO-$PbF_2$ flux. In the X-ray diffraction analysis, PZT(52/48) thick films showed a perovskite polycrystalline structure without a pyrochlore phase.

• 한국산업보건학회지
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• 제5권2호
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• pp.212-225
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• 1995

This study was performed in a diatomite factory located at Pohang City, Kyeongsangbuk-Do. The major objectives were to evaluate sampling and analytical methods of diatomaceous earth dust. Concentrations of total and respirable diatomaceous earth dust were measured. Size distribution of dust was analyzed by a personal cascade impactor and the particle size analyzer which is an application of multiple diffraction method. Also crystalline silica in respirable and total dust samples was analyzed quantitatively by X-ray diffraction and Fourie Transform Infrared Spectroscopy(FTIR). The results were as follows: The airborne total and respirable dust concentrations, particle size distribution, and cristalline silica(quartz) concentrations showed approximately a log-normal distribution. The means of totaldust concentrations at flour maufacturing, fire brick grinding and packaging processes exceeded the Korean and American Conference of Governmental Industrial Hygienists standards, $10mg/m^3$. The size distribution of diatomaceous earth dust was log-normal and identified as the rspirable particle mass and thoracic particle mass. The crystalline silica in respirable and total dust samples was identified to quartz and contained about 10 % in those samples. Finally, it is necessary to study the applicability of multiple diffraction for particle size distribution to compare the ACGIH's size selective sampling with other materials containing crystalline silica. Also, advanced quantitative study to X-ray diffraction and FTIR methods shoud be carried out 10 verify general and specific characteristics for respirable crystalline silica.

• Nuclear Engineering and Technology
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• 제54권3호
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• pp.1062-1070
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• 2022

In the present communication, pure and stable α-Bismuth Oxide (Bi₂O₃) nanoparticles (NPs) were synthesized by low temperature solution combustion method using urea as a fuel and calcined at 500℃. The synthesized sample was characterized by using powder X-ray Diffraction (PXRD), Scanning Electron Microscopy (SEM), Energy dispersive X-ray analysis (EDAX), Transmission Electron Microscopy (TEM), Fourier Transform Infrared Spectroscopy (FTIR) and UV-Visible absorption spectroscopy. The PXRD pattern confirms the formation of mono-clinic, stable and low temperature phase α-Bi₂O₃. The direct optical energy band gap was estimated by using Wood and Tauc's relation which was found to be 2.81 eV. The characterized sample was studied for X-ray/gamma ray shielding properties in the energy range 0.081-1.332 MeV using NaI (Tl) detector and multi channel analyzer (MCA). The measured shielding parameters agrees well with the theory, whereas, slight deviation up to 20% is observed below 356 keV. This deviation is mainly due to the influence of atomic size of the target medium. Furthermore an accurate theory is necessary to explain the interaction of X-ray/gamma ray with the NPs.The present work opens new window to use this facile, economical, efficient, low temperature method to synthesize nanomaterials for X-ray/gamma ray shielding purpose.

• Bulletin of the Korean Chemical Society
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• 제17권7호
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• pp.643-647
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• 1996

1,2-Disubstituted chiral calix[4]arene "25-(3,5-dinitrobenzoyloxy)-26-methoxy-27,28-dihydroxycalix[4]arene" was synthesized by the reaction of 25-(3,5-dinitrobenzoyloxy)-calix[4]arene with methyl iodide in the presence of K2CO3. Methylation was occurred at the 26-position of calix[4]arene. The partial cone conformation and 1,2-substitution were characterized based on the 1H NMR, 13C NMR and X-ray diffraction analysis. The crystal structure has been determined by X-ray diffraction method. The crystals are orthorhombic, Pbca, a=10.652(1), b=17.687(1), c=32.247(3) Å, Z=8, V=6075.4(9) Å3, Dc=1.38gcm-3. The intensity data were collected on an Enraf-Nonius CAD-4 Diffractometer with a graphite monochromated Cu-Kα radiation. The structure was solved by direct method and refined by full-matrix least-squares methods to a final R value of 0.050 for 2368 observed reflections. The molecule is in the partial cone conformation. It has two strong intramolecular hydrogen bonds of O(1D)-H…O(1C)-H…O(1B).

• Nuclear Engineering and Technology
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• 제4권1호
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• pp.31-34
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• 1972

X-선회절 실험에서 불필요한 관측치에 대한 실제실험치의 비율을 높이기 위한 역격자공간방법을 중성자의 경우에 응용하고 여러가지 실험방법을 택하는 경우에 적합한 검출기의 크기에 대한 관계식을 도출하였다.